Gh. Zgherea/Chem.J. Mold. 2008, 3 (1),52-55two mixture <strong>of</strong> binary phase that assure liquid-chromatographic separation, with a good resolution, for the syntheticallymixtures <strong>of</strong> 2.4-DNPH-ones provided by the carbonyl compounds with 2-4 atoms <strong>of</strong> carbon.2. The binary mixtures <strong>of</strong> mobile phase, obtained by the programs GBMP and GBMP , assure a better separationI II<strong>of</strong> synthetic mixtures witch contain the derivate compounds <strong>of</strong> inferior carbonyl compounds; in these synthetic mixturesthe ratio between 2.4DNPHAA and 2.4-DNPHD is higher than one, but very low.3.In the case <strong>of</strong> natural mixtures <strong>of</strong> 2.4-DNPH-ones, similarly with synthetic mixtures, the binary mixtures<strong>of</strong> mobile phase <strong>of</strong>fer only partially analytical satisfaction. Thus, the figure 5 contains evident the dominant peak <strong>of</strong>2.4-DNPHAA. Using his surface value for quantitative appreciation by external standard method, obtain experimentalvalues accordingly with the literature, namely 15 mg·L -1 acetic aldehyde [6]. In the same chromatogram, the peak <strong>of</strong>2.4DNPHD there is the second, but the second one is on the tailing peak <strong>of</strong> the first one. On the natural mixture <strong>of</strong>2.4DNPH-ones on might make the following consideration: if the literature <strong>of</strong>fer the real concentration values for thetwo carbonyl compounds, the accuracy <strong>of</strong> analytical system will justified by the big value, ~100, <strong>of</strong> the ratio between thequantities <strong>of</strong> acetic aldehyde and diacetyl. In this instance, the little peak <strong>of</strong> 2.4-DNPHD appears as a tailing peak on thebig peak <strong>of</strong> 2.4-DNPHAA, thus, his surface is higher than the normal one; the mistake value <strong>of</strong> surface chromatographicsignal became a source <strong>of</strong> mistake value <strong>of</strong> concentration.4.Each chromatogram – figures 2, 4, and 5 - contains any signals with lower values <strong>of</strong> retention time; it is thesignals for solvent.ExperimentalSolvents and mobile phasesThe acetonitrile was utilized to solve the pure 2.4-DNPH-ones. To liquid-chromatographic separations wasutilized two binary gradient mixtures <strong>of</strong> mobile phase – GBMP Iand GBMP II– with water (2 S·cm -1 ) and methanol(Merck).The synthetic mixtures <strong>of</strong> 2.4-DNPH-onesThe pure 2.4-DNPH-ones – yellow powders - are obtained in our laboratory, using 2.4-DNPH and chemicalpure carbonyl compound; thus: 2,4-DNPHAA (acetic aldehyde), 2.4-DNPHD (diacetyl), 2.4-DNPHA (acetone),2.4-DNPHP (propanal) and 2.4-DNPHiBA (isobutyl aldehyde). Their purity was verified by: elemental analysis, IRspectrophotometry and liquid-chromatographic separations. In acetonitrile (Merck, pro liquid chromatography) wereobtained 5·10 -4 M solutions. By controlled mixing was obtained two synthetic mixtures, abbreviated SM Iand SM II; theratio between the quantities 2.4-DNPHAA and 2.4-DNPHD is higher to one, in each mixture.The natural mixtures <strong>of</strong> 2.4-DNPH-onesThe carbonyl compounds from beer were separate by distillation on the water bath and transferred in 2.4DNPH,acid solution; the precipitates form a natural mixture <strong>of</strong> 2.4-DNPH-ones. They are isolated by filtration, washing withpure water, drying and solved in acetonitrile.ApparatusFor the separations was utilized Pye Unicam Philips liquid chromatograph, equipped with: an installation fordegassation <strong>of</strong> mobile phase (by refluxation) [7], gradient programmer for mobile phase (type LC-XPD, able to mixtwo liquids), separation columns with gradient <strong>of</strong> stationary phase, installation for column thermostatation, electronicintegrator (type DP101) and potentiometric recorder (type PM8251). The mixing program <strong>of</strong> liquids has nine segments<strong>of</strong> time, g=1-9; each timing segment has independent dimension <strong>of</strong> 0-99 minutes. In every moment, the value <strong>of</strong> B, thepercent <strong>of</strong> the second component in the mixture <strong>of</strong> mobile phase (A + B=100), is% B = k · t n (1)where, t – dimension <strong>of</strong> timing segment (minutes), k – slope <strong>of</strong> curve (describes the evolution <strong>of</strong> B value on the tsegment), n – exponent, with values 0.0-9.9 (describes the geometry <strong>of</strong> mixing curve).References[1] Simion Gocan, Cromatografie de Înalt Performan, Partea a II-a, Cromatografia de Lichide pe Coloane, EdituraRISOPRINT, Cluj-Napoca, 2002, pp 173-183.[2] Douglas A. Skoog, Principles <strong>of</strong> Instrumental Analysis, Third edition, Saunders College Publishing, 1985, pp801-815.[3] Candin Liteanu; Simion Gocan; T. Hodisan; H. Nascu, Cromatografia de Lichide, Editura Stiintifica, Bucuresti,1974, pp 156-157.[4] Radu Bacaloglu; Carol Csunderlik ; Livius Cotarc; Hans-Horst Glatt, Structura i Proprietile CompuilorOrganici, volumul I, Editura Tehnic, Bucureti, 1985, pp 116-127.[5] Gort S.M., Hogendoorn E.A.; Dijkman E.; Van Zoonen P.; R. Hoogerbrugge, The Optimisation <strong>of</strong> Step-GradientElution Conditions in Liquid Chromatography, Chromatographia, vol. 42, No ½, ian 96, pp 17-24.[6] *** BIERANALYSE 9.11 Bestimmung der Gärungsneben produkte in Bier, pp 246-250.[7] Gheorghe Zgherea, Installation to Continuously Degassation by Refluxing <strong>of</strong> Mobile Phases for HPLC, Annals <strong>of</strong>West University <strong>of</strong> Timioara, series Chemistry 12 (3) (2003) pp 1157-1160.55
Chemistry Journal <strong>of</strong> Moldova. G. Vasile General, et al./Chem.J. Industrial Mold. and 2008, Ecological 3 (1), 56-61 Chemistry. 2008, 3 (1), 56-61STUDY ON QUANTITATIVE SPECIATION, BY BCR METHOD, OF ZINCCONTENT FROM RIVER SEDIMENTSGeorgiana Vasile*, Stanescu Bogdan, Tudor Claudia, Elena MihailaNational Research and Development Institute for Industrial Ecology – ECOIND 90-92 Panduri Road, 050663,Bucharest, sector 5, Romania*Corresponding author: phone: +40/21/4100377; fax: +40/21/4100575; e-mail: ecoind@incdecoind.roKeywords: sediment, sequential extraction, bioavailability, zinc mobility.An unwanted consequence <strong>of</strong> human activity and <strong>of</strong> uncontrolled industrialization is the environment contaminationwith a lot <strong>of</strong> pollutants, among them heavy metal anthropogenic pollution having some most serious consequences. Areliable estimation <strong>of</strong> pollution level is made by studying heavy metal concentrations in the sediments.In our study the zinc content <strong>of</strong> the water and river sediments has been investigated, in an area polluted bymining activities, to provide information on the mobility and availability <strong>of</strong> this element. Sediment and water sampleshave been collected from significant sites in a former mining area in which with some sterile pits, which represent amajor environmental hazard.The zinc mobility and bioavailability in the environment was investigated by the three-step sequential extractionprocedure, a protocol proposed by the Standards, Measurements and Testing programme (SM & T–formerly BCR)<strong>of</strong> the European Union. The BCR sequential extraction scheme has the advantage that there are reference materialsavailable with certified and indicative values for the concentrations <strong>of</strong> selected elements in the particular extractionsteps. The BCR procedure enables fractionalization <strong>of</strong> metal content into the following fractions:EASILY MOBILIZABLE FRACTION: This fraction contains the specifically bound, surface occluded species(sometimes also CaCO3 bound species and metallo-organic complexes with low bonding forces).ORGANICALLY BOUND FRACTIONMn-Fe-and Al-OXIDE BOUND FRACTIONRESIDUAL FRACTION: This fraction mainly contains crystalline-bound trace metals and is most commonlydissolved with high concentrated acids and special digestion procedures.Combination <strong>of</strong> data from sequential extraction procedures and normalisation approaches provides a good basisto estimate the proportions <strong>of</strong> the easily and sparingly soluble metal fractions in the samples investigated and to identifythe anthropogenic input <strong>of</strong> metals into the environment.IntroductionFrom the pollution types that are to be found in our country, the most prevalent and having powerful effects forthe quality <strong>of</strong> surface waters and <strong>of</strong> the sediments, is the heavy metals pollution that is to be found especially in the areashaving a long ores extraction activity.Understanding the importance <strong>of</strong> sediments role in contaminants transport and storage, conduced to an increasingpreoccupation <strong>of</strong> the researchers and <strong>of</strong> the organisms responsible for the control and the prevention <strong>of</strong> water pollution,in the pollutant compounds knowledge field.For an evaluation <strong>of</strong> heavy metals charge in the sediments, is not sufficient to determinate their total concentration.The establishment <strong>of</strong> the metals proportions in easy soluble fractions and in the hard soluble ones is very important.These fractions evaluation allows the elucidation <strong>of</strong> their existing dangers and seriousness for the aquaticecosystems [1].The signification <strong>of</strong> speciation analyze as a method for estimating the environment risk was recognized by theEnvironment Conservation Council from Australia and New Zeeland (ANEZECC), who recommanded the examination<strong>of</strong> bioaccesible concentrations, where the metals total levels overpass the levels established into the Interimare QualityCriteria for Sediments[2].For the estimation <strong>of</strong> the natural and the anthropogenic inputs <strong>of</strong> the heavy metals in the sediments, are usedidentification methods by sequential chemical extraction (BCR technique) and normalizations, based on the correlationsbetween the concentrations <strong>of</strong> the elements present in the tracks, and an element that is naturally present in theinvestigated environment [3].Further on are presented the results <strong>of</strong> the researches effectuated on sediments sampled from Certej River,which is affected by the long ore extraction activities. The papers that present the results in the thematic approach weredirected towards zinc content knowledge and towards the quantification <strong>of</strong> its existing forms in sediments.56
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